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A kind of production method of laurolactam

A technology of laurolactam and cyclododecanone is applied in the production field of high-purity laurolactam, and achieves the effects of being difficult to agglomerate, being convenient for packaging, storage and transportation, and being easy to realize.

Active Publication Date: 2020-11-24
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The purpose of the present invention is to provide a method for producing high-purity laurolactam, which solves the problem of oximation reaction rate, the problem of heavy discharge heat and the purification of laurolactam products

Method used

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  • A kind of production method of laurolactam
  • A kind of production method of laurolactam
  • A kind of production method of laurolactam

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Embodiment 1

[0043] Step 1: 180 g of an aqueous solution of hydroxylamine sulfate (12.5 wt %) was added to ammonia water to neutralize to pH 6-7 to obtain a hydroxylamine solution. In the round bottom bottle, 100 g of cyclododecanone was heated and melted, kept at 90° C., and the aforementioned hydroxylamine solution was added dropwise into the round bottom bottle while stirring. The dropwise addition time is about 10 minutes. After the dropwise addition is completed, the reaction is continued for 1 hour, and then 100 g of 1-cyclohexyl-n-tridecane is added for liquid separation. The oil phase obtained after liquid separation contained 0.2% water and 100 ppm inorganic salt.

[0044] Step 2: The above-mentioned oil phase is subjected to vacuum rectification, and cyclododecanone is distilled under the conditions of pressure 1kPa, temperature 110°C, and the number of theoretical plates in the rectification column is not less than 20. About 45 g of cyclododecanone was obtained, with a purity o...

Embodiment 2

[0067] Step 1: 100 g of an aqueous solution of hydroxylamine sulfate (12.5 wt %) was added to ammonia water to neutralize to pH 6-7 to obtain a hydroxylamine solution. In the round bottom bottle, 100 g of cyclododecanone was heated and melted, kept at 90° C., and the aforementioned hydroxylamine solution was added dropwise into the round bottom bottle while stirring. The dropwise addition time is about 10 minutes. After the dropwise addition is completed, the reaction is continued for 1 hour, and then 120 g of 4-isopropyl-n-decylcyclohexane is added for liquid separation. The oil phase obtained after liquid separation contained 0.15% of water and 80 ppm of inorganic salts.

[0068] Step 2: The above-mentioned oil phase is subjected to vacuum rectification, and cyclododecanone is distilled under the conditions of pressure 1kPa, temperature 110°C, and the number of theoretical plates in the rectification column is not less than 20. About 65 g of cyclododecanone was obtained, wi...

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Abstract

The invention relates to a method for producing high-purity laurolactam, which comprises using cyclododecanone as a raw material, reacting with hydroxylamine, adding solvent a to assist liquid separation; the oil phase obtained by liquid separation is recovered by vacuum distillation The remaining cyclododecanone, and the solution rich in cyclododecanone oxime is mixed with concentrated sulfuric acid, and a Beckmann rearrangement reaction occurs. After the reaction, the mixed solution is neutralized with ammonia water, and the laurolactam a solution is obtained after liquid separation , after the impurities are adsorbed by alumina, solvent b is added, and the solid product of laurolactam is obtained by cooling and crystallizing in the solution of the mixed solvent of a and b. The laurolactam product obtained by the method has high purity and light color, and is suitable for producing high-grade resin materials.

Description

technical field [0001] The invention relates to a production method of laurolactam, in particular to a production method of high-purity laurolactam. Background technique [0002] Lauryl lactam is an important chemical raw material for the production of high-performance nylon material - nylon 12. [0003] In industry, laurolactam is obtained from cyclododecanone as raw material through oximation reaction and Beckmann rearrangement reaction. Although in terms of chemical reaction form, the production of laurolactam from cyclododecanone and the production of caprolactam from cyclohexanone are similar. However, since the physical and chemical properties of cyclododecanone and its corresponding derivatives are significantly different from those of cyclohexanone and its corresponding derivatives, the difficulty of producing laurolactam is obviously increased, and many problems still exist in the existing technology. [0004] First, the oximation reaction process is complex and t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D201/06C07D225/02
Inventor 张彦雨陈海波杜旺明边新建赵晶黎源孟熙王文
Owner WANHUA CHEM GRP CO LTD
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